CN103553153B - Method and device for continuously synthesizing spherical nickel hydroxide - Google Patents
Method and device for continuously synthesizing spherical nickel hydroxide Download PDFInfo
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- CN103553153B CN103553153B CN201310522773.1A CN201310522773A CN103553153B CN 103553153 B CN103553153 B CN 103553153B CN 201310522773 A CN201310522773 A CN 201310522773A CN 103553153 B CN103553153 B CN 103553153B
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Abstract
The invention provides a method for continuously synthesizing spherical nickel hydroxide. The method comprises the following steps: 1, adding a nickel sulfate solution, a sodium hydroxide solution and an ammonium hydroxide solution into a pipeline synthesizer through a metering pump so as to perform a synthetic reaction; 2, enabling the solution after the synthetic reaction to automatically flow into the kettle body of a synthesis aging filtration washing kettle so as to perform a synthesis aging reaction on the nickel hydroxide; 3, filtering a reaction solution with a microporous filtering pipe so as to continuously pump out the sodium sulfate solution; 4, washing a concentrate in the synthesis aging filtration washing kettle so as to obtain a nickel hydroxide concentrate; and 5, performing solid-liquid separation on the nickel hydroxide concentrate so as to obtain the spherical nickel hydroxide. The method can realize continuous production and has a short process, thereby being especially suitable for preparing the spherical nickel hydroxide. The method has the advantages of continuous production, short process, good spherical nickel hydroxide appearance, small equipment occupation area, low energy consumption and small investment. In addition, the invention further provides a device for continuously synthesizing the spherical nickel hydroxide.
Description
Technical field
The invention belongs to the synthesis field of ball-shape nickel hydroxide, be specifically related to a kind of method and device of ball-shape nickel hydroxide continuous synthesis.
Background technology
Ball-shape nickel hydroxide is the positive electrode material of nickel metal hydride battery and Ni-H 2 power accumulator, also can be used as the front body material of anode active material of lithium ion battery (lithium nickel cobalt dioxide) simultaneously.The scale operation of high performance spherical nickel hydroxide, to the development promoting the industry such as domestic mobile communication and electromobile, reduces topsoil, improves the aspects such as environment for human survival all significant.
At present, the preparation of ball-shape nickel hydroxide is generally adopt reactor, aging reactor, two-in-one filter or the equipment such as whizzer, homogenizing still to realize preparation and the thickening and washing process of ball-shape nickel hydroxide, there is batch production, technical process is long, energy consumption is high, has the problems such as certain destruction, occupation area of equipment is large, investment cost is high to the microscopic appearance of ball nickel product in implementation process.
Summary of the invention
For overcoming the problems such as the technical process existed in prior art is long, occupation area of equipment is large, investment cost is high, energy consumption is high, the invention provides a kind of method of ball-shape nickel hydroxide continuous synthesis; The present invention additionally provides a kind of device of ball-shape nickel hydroxide continuous synthesis simultaneously.
The present invention is achieved through the following technical solutions:
A method for ball-shape nickel hydroxide continuous synthesis, is characterized in that, comprises the following steps:
The first step: the ratio of ammonia soln according to throughput ratio 1:0.6:0.2 of to be the sodium hydroxide solution of 8 ~ 10 M and volumetric molar concentration by the nickel sulfate solution of 118 ~ 122 g/l, volumetric molar concentration be 10 ~ 12M, joins pipeline synthesizer by volume pump according to the flow of nickel sulfate solution 300 ~ 400 ls/h and carry out building-up reactions;
Second step: the solution after building-up reactions is flowed automatically in the kettle of synthesis ageing filtration washing still, be provided with whipping appts, microfiltration tube and guide shell in described kettle; Open described whipping appts, carry out the synthesis ageing reaction of 6 ~ 8 hours nickel hydroxides;
3rd step: vacuumize in the process of synthesis ageing reaction, adopts microfiltration tube to filter reaction solution simultaneously, is constantly extracted out by metabisulfite solution;
4th step: after the pH value of the nickel hydroxide slurries in synthesis ageing thickening and washing still reaches 12 ~ 13, adopts hot pure water to the concentrated solution washing in synthesis ageing thickening and washing still 3 ~ 4 times, obtains nickel hydroxide concentrated solution;
5th step: nickel hydroxide concentrated solution is carried out solid-liquor separation, obtains ball-shape nickel hydroxide.
Further, the pH value delta data by adopting the mode of installing online PH meter in synthesis ageing thickening and washing still to observe solution in the 4th step.
The present invention also provides a kind of device of ball-shape nickel hydroxide continuous synthesis simultaneously, comprise reactor and synthesis ageing filtration washing still, liquid ammonia storage tank, sodium hydroxide solution storage tank are connected with reactor respectively by three pipelines with nickel sulfate solution storage tank, and described every root pipeline is provided with a volume pump; The delivery port of reactor is communicated with the fluid inlet of synthesis ageing filtration washing still; Described synthesis ageing filtration washing still inside is provided with whipping appts, microfiltration tube and guide shell; The first via delivery port of synthesis ageing filtration washing still is connected with whizzer with valve through nickel hydroxide concentrated solution transferpump, and the second road delivery port of synthesis ageing filtration washing still is connected with vacuum pump through surge tank; The first via input aperture of synthesis ageing filtration washing still is connected with pure water source, and the second input aperture, tunnel of synthesis ageing filtration washing still is connected with air compressor with water-and-oil separator through air accumulator.
Further, described whipping appts stretches into the central position of kettle from synthesis ageing filtration washing still outside, and guide shell is set in the periphery of whipping appts; Described microfiltration tube is arranged on the periphery of guide shell.
The method of ball-shape nickel hydroxide continuous synthesis of the present invention can realize continuous seepage, and technical process is short, synthesis ageing thickening and washing all completes in washing kettle, be particularly suitable for the preparation of ball-shape nickel hydroxide, the present invention has continuous seepage, technical process is short, product pattern is good, occupation area of equipment is few, energy consumption is low, invest low advantage.
Below in conjunction with accompanying drawing, the present invention will be further described.
Accompanying drawing explanation
Fig. 1 is the structural representation of device of the present invention;
Fig. 2 is the structure iron of synthesis ageing filtration washing still;
In figure, the implication of each label is as follows:
1, liquid ammonia storage tank 2, volume pump 3, sodium hydroxide solution storage tank 4, nickel sulfate solution storage tank 5, nickel sulfate solution 6, sodium hydroxide solution 7, ammoniacal liquor 8, reactor 9, nickel hydroxide concentrated solution 10, whipping appts 11, microfiltration tube 12, guide shell 13, synthesis ageing filtration washing still 14, nickel hydroxide concentrated solution transferpump 15, valve 16, whizzer 17, pure water source 18, air compressor 19, water-and-oil separator 20, air accumulator 21, high pressure gas 22, metabisulfite solution 23, surge tank 24, air 25, vacuum pump.
Embodiment
As shown in Figure 1, 2, the invention provides a kind of device of ball-shape nickel hydroxide continuous synthesis, comprise reactor 8 and synthesis ageing filtration washing still 13, liquid ammonia storage tank 1, sodium hydroxide solution storage tank 3 are connected with reactor 8 respectively by three pipelines with nickel sulfate solution storage tank 4, and described every root pipeline is provided with a volume pump 2; The delivery port of reactor 8 is communicated with the fluid inlet of synthesis ageing filtration washing still 13.
Described synthesis ageing filtration washing still 13 inside is provided with whipping appts 10, microfiltration tube 11 and guide shell 12; Described whipping appts 10 stretches into the central position of kettle from synthesis ageing filtration washing still 13 outside, and guide shell 12 is set in the periphery of whipping appts 10; Described microfiltration tube 11 is arranged on the periphery of guide shell 12.The first via delivery port of synthesis ageing filtration washing still 13 is connected with whizzer 16 with valve 15 through nickel hydroxide concentrated solution transferpump 14, and the second road delivery port of synthesis ageing filtration washing still 13 is connected with vacuum pump 25 through surge tank 23; The first via input aperture of synthesis ageing filtration washing still 13 is connected with pure water source 17, and the second input aperture, tunnel of synthesis ageing filtration washing still 13 is connected with air compressor 18 with water-and-oil separator 19 through air accumulator 20.Wherein, described microfiltration tube 11 acid-and base-resisting chemical regeneration, the pressurized gas of resistance to 0.7MPa or clear water pulse cleaning.
Adopt the device of above-mentioned ball-shape nickel hydroxide continuous synthesis to carry out the method for ball-shape nickel hydroxide continuous synthesis, comprise the following steps:
The first step: the ratio of ammonia soln according to throughput ratio 1:0.6:0.2 of to be the sodium hydroxide solution of 8 ~ 10 M and volumetric molar concentration by the nickel sulfate solution of 118 ~ 122 g/l, volumetric molar concentration be 10 ~ 12M, joins pipeline synthesizer by volume pump according to the flow of nickel sulfate solution 300 ~ 400 ls/h and carry out building-up reactions;
Second step: flowed automatically to by the solution after building-up reactions in the kettle of synthesis ageing filtration washing still, open described whipping appts, under the acting in conjunction of whipping appts and guide shell, carries out the synthesis ageing reaction of 6 ~ 8 hours nickel hydroxides;
3rd step: adopt vacuum extractor to vacuumize kettle in the process of synthesis ageing reaction, adopts microfiltration tube to filter reaction solution simultaneously, is constantly extracted out by metabisulfite solution, reach the object of continuous concentration nickel hydroxide slurries.
4th step: by the pH value delta data adopting the mode of installing online PH meter in synthesis ageing thickening and washing still to observe solution, after the pH value of the nickel hydroxide slurries in synthesis ageing thickening and washing still reaches 12 ~ 13, open hot pure water device, adopt hot pure water to the concentrated solution washing in synthesis ageing thickening and washing still 3 ~ 4 times, obtain nickel hydroxide concentrated solution;
5th step: nickel hydroxide concentrated solution is carried out solid-liquor separation, obtains ball-shape nickel hydroxide.
The present invention is not only confined to above-mentioned embodiment; persons skilled in the art are according to content disclosed by the invention; other multiple embodiment can be adopted to implement the present invention; therefore; every employing project organization of the present invention and thinking; do the design that some simply change or change, all fall into the scope of protection of the invention.
Claims (3)
1. a method for ball-shape nickel hydroxide continuous synthesis, is characterized in that, comprises the following steps:
The first step: the ratio of ammonia soln according to throughput ratio 1:0.6:0.2 of to be the sodium hydroxide solution of 8 ~ 10 M and volumetric molar concentration by the nickel sulfate solution of 118 ~ 122 g/l, volumetric molar concentration be 10 ~ 12M, joins pipeline synthesizer by volume pump according to the flow of nickel sulfate solution 300 ~ 400 ls/h and carry out building-up reactions;
Second step: the solution after building-up reactions is flowed automatically in the kettle of synthesis ageing filtration washing still, be provided with whipping appts, microfiltration tube and guide shell in described kettle; Open described whipping appts, carry out the synthesis ageing reaction of 6 ~ 8 hours nickel hydroxides;
3rd step: vacuumize in the process of synthesis ageing reaction, adopts microfiltration tube to filter reaction solution simultaneously, is constantly extracted out by metabisulfite solution;
4th step: after the pH value of the nickel hydroxide slurries in synthesis ageing thickening and washing still reaches 12 ~ 13, adopts hot pure water to the concentrated solution washing in synthesis ageing thickening and washing still 3 ~ 4 times, obtains nickel hydroxide concentrated solution;
5th step: nickel hydroxide concentrated solution is carried out solid-liquor separation, obtains ball-shape nickel hydroxide;
The device that aforesaid method adopts comprises reactor (8) and synthesis ageing filtration washing still (13), liquid ammonia storage tank (1), sodium hydroxide solution storage tank (3) are connected with reactor (8) respectively by three pipelines with nickel sulfate solution storage tank (4), and described every root pipeline is provided with a volume pump (2); The delivery port of reactor (8) is communicated with the fluid inlet of synthesis ageing filtration washing still (13); Described synthesis ageing filtration washing still (13) inside is provided with whipping appts (10), microfiltration tube (11) and guide shell (12); The first via delivery port of synthesis ageing filtration washing still (13) is connected with whizzer (16) with valve (15) through nickel hydroxide concentrated solution transferpump (14), and the second road delivery port of synthesis ageing filtration washing still (13) is connected with vacuum pump (25) through surge tank (23); The first via input aperture of synthesis ageing filtration washing still (13) is connected with pure water source (17), and the second input aperture, tunnel of synthesis ageing filtration washing still (13) is connected with air compressor (18) with water-and-oil separator (19) through air accumulator (20).
2. the method for ball-shape nickel hydroxide continuous synthesis according to claim 1, is characterized in that, the pH value delta data by adopting the mode of installing online pH meter in synthesis ageing thickening and washing still to observe solution in the 4th step.
3. the method for ball-shape nickel hydroxide continuous synthesis according to claim 1, it is characterized in that, described whipping appts (10) stretches into the central position of kettle from synthesis ageing filtration washing still (13) outside, and guide shell (12) is set in the periphery of whipping appts (10); Described microfiltration tube (11) is arranged on the periphery of guide shell (12).
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| CN104319394A (en) * | 2014-10-17 | 2015-01-28 | 金川集团股份有限公司 | Method for preparing pure-phase spherical nickel hydroxide |
| CN105355902A (en) * | 2015-11-23 | 2016-02-24 | 兰州金川新材料科技股份有限公司 | Preparation method for continuously synthesizing lithium ion positive electrode material precursor |
| CN106587177A (en) * | 2016-12-30 | 2017-04-26 | 江门市崖门新财富环保工业有限公司 | Technology for nickel ball production and byproduct recovery |
| CN108461749B (en) * | 2018-06-04 | 2024-02-13 | 浙江东瓯过滤机制造有限公司 | Ternary precursor production optimization control device and optimization control method thereof |
| CN110803722A (en) * | 2018-08-06 | 2020-02-18 | 天津市茂联科技有限公司 | Preparation method of large-particle nickel hydroxide |
| CN115582082B (en) * | 2022-10-18 | 2023-10-27 | 长春生物制品研究所有限责任公司 | System and process for producing aluminum hydroxide adjuvant based on-line detection and control system |
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| CN1281512C (en) * | 2004-03-31 | 2006-10-25 | 北京有色金属研究总院 | Method for continuously preparing nickelous hydroxide |
| CN1301776C (en) * | 2005-03-22 | 2007-02-28 | 温州市东瓯微孔过滤有限公司 | Filtration and washing technology in preparing metal or non metal fine granular powder |
| CN203602368U (en) * | 2013-10-28 | 2014-05-21 | 浙江东瓯过滤机制造有限公司 | Spherical nickel hydroxide continuous synthesis device |
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Denomination of invention: A Method and Device for Continuous Synthesis of Spherical Nickel Hydroxide Effective date of registration: 20221213 Granted publication date: 20150107 Pledgee: Agricultural Bank of China Limited Lishui Development Zone Sub branch Pledgor: ZHEJIANG DONGOU FILTER MANUFACTURING Co.,Ltd. Registration number: Y2022330003660 |
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